Category: 1544-75-8

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 1544-75-8, name is 5-Fluoro-1H-benzo[d]imidazol-2(3H)-one, A new synthetic method of this compound is introduced below., Recommanded Product: 1544-75-8

Obtained through a method the N- acetyl benzylamine piperazine (II) intermediate (19. 6mmol), an alcoholic solution of formaldehyde (16. 3mmol), 5- fluoro-1,3-dihydro-benzimidazol-2-one (16. 3mmol) into 30ml of absolute ethanol, at room temperature for 15h. The reaction was concentrated under reduced pressure to give a crude oil. The crude product was purified by silica gel column chromatography to obtain the free base of N- benzyl-2- {4 – [(5-fluoro-2-oxo-2,3-dihydro-benzo -111- [(1] imidazol-1 yl) methyl] piperazin-1-yl} acetamide (V_19), 4.67g, yield 72.1%.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Shanghai Pharmaceutical Industry Research Academy; China State Institute of Pharmaceutical Industry; Li, Jiangqi; Weng, Zhije; Cui, Ning; Jie, Peng; Ma, Xiao; (25 pag.)CN105418506; (2016); A;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem

Electric Literature of 1544-75-8, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 1544-75-8 as follows.

[00312] lodomethane (0.82 mL, 13.15 mmol) was added to a mixture of 5-fluoro-1,3-dihydro-2H-benzimidazol-2-one (500. mg, 3.29 mmol) and potassium carbonate (1.81 g, 13.15mmol) in DMF (25 mL), and the reaction mixture stirred at ambient temperature for 16 h. DCM(30 mL) and water (60 mL) were added and the mixture stirred for 5 min. The DCM layer wasisolated by passing through a hydrophobic frit and the aqueous washed with DCM (2 x 50mL). The combined DCM extracts were concentrated under reduced pressure to yield 5-fluoro-1,3-dimethyl-benzimidazol-2-one (556 mg, 2.99 mmol, 91%).[00313] 1H NMR (300MHz, CDCI3) 5 = 6.91 – 6.71 (m, 3H), 3.42 (s, 3H), 3.41 (s, 3H)

According to the analysis of related databases, 1544-75-8, the application of this compound in the production field has become more and more popular.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 1544-75-8, name is 5-Fluoro-1H-benzo[d]imidazol-2(3H)-one, A new synthetic method of this compound is introduced below., Recommanded Product: 1544-75-8

A solution of 5-fluoro-1 H-benzo[d]imidazol-2(3H)-one (16.0 g, 105 mmol) in DMF (400 mL) under nitrogen was cooled with an ice-bath, using a mechanical stirrer for agitation. It was then treated over 10 min with sodium hydride (60% w/w in mineral oil, 13.1 g, 327 mmol) and the resulting mixture was stirred at this temperature for 30 min before being treated with iodomethane (26.3 mL, 422 mmol) over 30 min. The resulting mixture was then allowed to warm to room temperature and after 1 h was carefully treated with water (500 mL). The aqueous phase was extracted with EtOAc (3 x 800 mL) and the combined organics were washed with brine (1 L), dried over MgS04 and concentrated in vacuo. Purification of the brown residue by flash chromatography on silica gel (SP4, 1.5 kg column, gradient: 0 to 25% (3: 1 EtOAc/EtOH) in cyclohexane) gave the title compound (15.4 g, 86 mmol, 81 %) as a pink solid. LCMS (high pH): Rt 0.76 min; [M+H+]+ = 181.1 deltaEta NMR (400 MHz, CDCI3) ppm 6.86-6.76 (m, 2H), 6.71 (dd, J = 8.3, 2.3 Hz, 1 H), 3.39 (s, 3H), 3.38 (s, 3H).

The synthetic route of 1544-75-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; BAMBOROUGH, Paul; CHUNG, Chun-Wa; LE GALL, Armelle; SHEPPARD, Robert John; (36 pag.)WO2016/62737; (2016); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem